HCID 69093719, compound → HCID 69094256, compound

Participants

Reaction Steps

To a solution of 143 (6 g, 11 mmol) in dichloromethane (120 mL) was added DMP (6.9 g, 16 mmol). The resulting solution was stirred for 1.5 hours at room temperature, then quenched by saturated aqueous sodium bicarbonate solution (80 mL), and extracted with dichloromethane (3×100 mL). The combined organic layer was washed with brine (2×50 mL), dried over anhydrous magnesium sulfate and concentrated under vacuum. The residue was purified by flash column chromatography with 5%-10% ethyl acetate in petroleum ether to afford 144 as a yellow syrup (4 g, 67%). (ES, m/z): [M+H]+ 553.0; 1H NMR (300 MHz, CDCl3): 7.34-7.19 (m, 10H), 6.10 (d, J=6.9 Hz, 1H), 5.85-5.76 (m, 1H), 5.10-4.94 (m, 2H), 4.69-4.25 (m, 7H), 4.15-4.10 (m, 1H), 3.97-3.83 (m, 2H), 2.19 (s, 3H), 1.50 (s, 9H).

Provenance & Evidence